Vitamin concentrate and process for producing same



Patented Mar. 14, 1939 UNiTED STATES VITAMIN CONCENTRATE AND PROCESS FORPRODUCING SAME Andre E. Briod, Belleville, and Bion R. East, EastOrange, N. .L, assignors to National Oil Products Company, Harrison, N.J., a corporation of New Jersey No Drawing. Original application July16, 1936, Serial No. 90,888. Divided and this application October 23,1937, Serial No. 170,582

8 Claims. (Cl. 99-11) This invention relates to a new method ofincorporating vitamin concentrates, particularly vitamins A and D, tomilk products and other food products.

It more particularly concerns itself with the preparation of so-calledvitamin D milk, the use and value of which have become well-known in thelast few years.

The discovery of vitamins has brought a wide spread use of variousproducts enriched with such vitamins; and, while the necessity of someof these products may be open to question, there is no such doubt inregard to vitamin D milk. With the approval of numerous medical andnutritional authorities, it has become firmly established as a food ofenhanced nutritional value, in which the specific virtues of milk andvitamin D are combined in a most useful manner.

While vitamin D milk can be produced by various methods, such asaddition of irradiated products to milk, direct irradiation, feeding ofirradiated and other vitamin D products to cows, etc., our invention hasto do with the production of vitamin D milk by the addition ofnaturallyoccurring vitamin concentrates to milk.

Cod liver oil has long been known to possess special therapeuticqualities, but it is only with the discovery of the oil-soluble vitaminsthat these qualities became fully understood. The further discovery thatthe vitamins were contained in the unsaponifiable fraction of cod liveroil and other fish liver oils led to new methods of administra tion ofthese vitamins. Their concentration is now well known and widelypracticed.

Such fish liver oil concentrates were first administered in tablet form,or dissolved to a desired strength in other oils such as corn oil. Whilethe improvement over the necessity of taking cod liver oil was great, itstill presented certain difficulties, particularly with young children.

Vitamin D milk, made with cod liver oil concentrates, was thereforeintroduced with the idea of overcoming these difiiculties, whileproviding an automatic source of vitamin D of known and controlledpotency. The close association of the vitamin with the calcium andphosphorus of the milk was also viewed as an added advantage in this newmethod of providing vitamin D in the daily diet.

The incorporation of cod liver oil concentrate to milk, particularly ona commercial scale, did

not prove as simple as it sounded, however. A method was finallydeveloped where the concentrate, which is a mixture of crystalline, gellike and liquid fractions practically free from saponifiableconstituents, was dissolved in a neutral oil, such as corn oil, to apredetermined vitamin potency. This standardized oil solution of theconcentrate was used by the dairies to make vitamin D milk in thefollowing manner:

A calculated amount of the oil solution of concentrate was measured andemulsified in a small portion of milk, using a suitable emulsifier orhomogenizer for this operation. The concentrated emulsion in milk wasthen mixed into the 1. whole batch, which was subsequently pasteurizedand bottled as usual.

The above method had some very serious drawbacks, chief among which maybe mentioned:

A. The concentrate had to be dissolved in a leneutral oil, thusnecessitating introduction into the milk of a substance foreign to theconcentrate or the milk.

B. The pre-emulsification oi' the oil solution of concentrate in themilk at the dairy was troublesome, and also unsatisfactory from asanitary standpoint.

C. The emulsification or homogenization in whole milk was not properlyeffective and prevented the milk from having a reasonably constantvitamin D potency throughout the batch. In addition to its separationwith the cream, the oil solution of concentrate would often separate asfree 011 globules on top of the milk, particularly after pasteurizationof the milk, which had the 3:

" effect of helping the separation and de-emulsification of the-addedoil solution of concentrate.

D. The oil used as a diluent would oxidize, with formation ofundesirable flavors both in the concentrate and in the milk, and withdetrimental effect on the vitamin A and D potency of the material. Y

E. The presence of the concentrate in the milk thus treated could bedetected by taste comparison with untreated milk. This was due to the 40ineifectiveness of the emulsification of the vitamin oil solution inwhole milk, together with the eifect of oxidation of the oil on thetaste of both the milk and the concentrate.

It can readily be seen that the above disadvantages were quite serious.Our new method has overcome all of these and has introduced otherdesirable features which have proved quite valuable to the art and whichhave greatly simplified the preparation of vitamin D milk withconcentrates from fish liver oils.

We have found that the direct homogenization of cod liver concentrate,without oil diluent, in evaporated milk or in cream, followed by canningand sterilization of the emulsion in scaled up cans, gave us a productwhich was eminently suited to the preparation of vitamin D milk.Contrary to our expectations, we found that the vitamin A and D potencyof the material was not affected by the sterilization of the material,which sterilization is required to keep it fresh indefinitely in thesealed can. The homogenization in evaporated milk or in cream was somuch superior to homogenization in whole milk that the stability of theemulsion was not disturbed by sterilization. This is apparently due tothe greater concentration of emulsifying ingredients in evaporated milkor in cream as against an equal amount of whole milk.

In addition, we have found that the stable sterilized emulsion thusproduced, when mixed in whole milk, remained evenly distributedthroughout the whole for 1* much longer period, instead of quicklyseparating with the cream of the milk. This is a distinct advantage fora material of this type, where it is sought to incorporate the vitaminpotency throughout the whole, particularly if some of the cream has tobe removed, as in the feeding of some young infants.

The finely divided nature of vitamin D in the product is also anadvantage and its close association with the calcium of the milk appearsto enhance its biological effect. Unit for unit, vitaminv D milk hasbeen shown to be superior to an equivalent amount of vitamin D in oildilution.

We have also found that, through some unexpected efiect of sterilizationin the presence of evaporated milk or cream on the taste of theconcentrate, which taste is distinctly modified, the resultingemulsified product gives a vitamin D milk which cannot be distinguishedfrom ordinary milk, even by experts on milk taste. This in itself is agreat improvement over results obtained in prior practice.

The ease of addition of this sterilized product to milk, with which itmixes very readily to form a homogeneous mass, has proved of great valueto the art, and the simplicity of th s new method is adequately shown inthe following example, which is given simply to illustrate one of itsmany applications:

Example Fifty gm. of a cod liver oil concentrate. consisting of therefined unsaponifiable portion of cod liver oil and containing 10.000 U.S. P. units of vitamin D and 50.000 U. S. P. units of vitamin A pergram. is homogenized with 950 gm. of freshly separated creamor with 950gm. of evaporated milk produced from whole milk by removal of half ofits water content. The emulsion is then canned, and the cans sealed andsterilized for twenty minutes at 242 F.

At the dairy. each 6 oz. can of the material will produce approximately213 quarts of vitamin D milk containing 400 U. S. P. units of vitamin Dper quart, and also an additional 2,000 U. S. P. units of vitamin A perquart. The vitamin D milk is obtained very simply by pouring thesterilized contents of the can in the 213 quarts of milk, mixing andpasteurizing as usual.

It is obvious that the proportion of concentrate in the canned emulsioncan vary within considerable limits. Usually, the strength can best bedetermined according to the quantity of vitamin D which it is desired toproduce daily. A large production, for example, will call for a producthaving the highest practical proportion of concentrate consistent withstability of the emulsion during and after sterilization. A smallproduction will call for a more dilute product, though an emulsioncontaining less than 100 U. S. P.

ent batches of concentrate will also modify thepercentage of concentrateneeded in an emulsion which is to have a predetermined vitamin Dpotency.

As a further desirable precaution to protect the vitamin potency andtaste of the material, the cans can be sealed under vacuum, afterremoval of air from the filled can.

The medium used for emulsiflcation of the concentrate can be changed tosuit special 'demand or special circumstances. It is possible, forexample, to make a reconstructed evaporated milk from milk powder and tohomogenize the concentrate therein, without departing from thecontemplatedscope of our invention. This reconstructed evaporated milk,made from milk powder to approximate the composition of evaporated milkmade from whole milk, also contains emulsifying ingredients in suitablestate and concentration for the production of a stable homogenized andsterilized emulsion of vitamin concentrate. It is therefore intendedthat our specification and claims, when they refer to evaporated milk,also include under that term the liquid carriers produced byredissolving milk powder to a composition approximating that ofevaporated milk made directly from whole milk by removal of part of itswater content. j

The concentrated emulsion can also be dried by suitable means, such asspray drying or drying over rollers. if a concentrated powdered productseems more desirable for addition of vitamin concentrate to powderedmilk, for example.

Other oils than cod liver oil can be used to produce the concentrate,and refined fish oils oi high vitamin A and D potency, such as tunaliver oil. can be used with or without further concentration of thevitamin potency. Concentrates which consist mainly of vitamin D fromfish liver oil can also be prepared by known methods and used in theperformance of our invention. While the use of vitamin concentratesobtained from marine oils is preferred; it is obvious that equivalentvitamin D and/or vitamin A and D concentrates, derived from othersources may be used in lieu of concentrates obtained from marine oils.

Furthermore, it is evident that our new products can also be used toincorporate vitamins A and D to foods other than milk, as for examplebread or other cereals, and to all preparations where the addition of aneasily dispersed emulsion of oil-soluble vitamins is adistinctadvantage.

By "milk product carrier" and milk product carriers in our specificationand claims, we

mean the products of the group consisting of cream and evaporated milkas hereinbefore qualified.

Since certain changes in carrying out the above process and certainmodifications in the composition which embody the invention may be madewithout departing from its scope. it is intended that all mattercontained in the above description shall be interpreted as illustrativeand not in a limiting sence.

This application is a division of our application for U. S. LettersPatent Serial Number 90,888, filed July 16, 1936.

Having described our invention, what we claim as new and desire tosecure by Letters Patent is:

1. A process for producing a vitamin D concentrate adapted for additionto foods, which consists in emulsifying vitamin D concentrate with amilk product carrier selected from the class consisting of cream andevaporated milk, canning and sterilizing the resulting emulsion.

2. A process for producing a vitamin A and D concentrate adapted foraddition to foods, which consists in emulsifying vitamin A and Dconcentrate with a milk product carrier selected from the classconsisting of cream and evaporated milk, canning the resulting emulsionand sterilizing the canned material. 3. A process for producing aconcentrate adapted for addition to foods, which consists in emulsifyingfish liver oil concentrate with a milk product carrier selected from theclass consisting of cream and evaporated milk, canning and sterilizingthe resulting emulsion.

4. A sterile vitamin D concentrate adapted for addition to foodsconsisting of a vitamin D concentrate uniformly dispersed in a milkproduct carrier selected from the group consisting 0 cream andevaporated milk. I

5. A sterile vitamin A and D concentrate adapted for addition to foodsconsisting of a vitamin A and D concentrate uniformly dispersed in amilk product carrier selected from the group consisting of cream andevaporated milk.

(5. A sterile concentrate adapted for addition to .foods consisting of afish liver oil concentrate uniformly dispersed in a milk product carrierselected from the group consisting of cream and evaporated milk.

7. A sterile vitamin D concentrate adapted for addition to whole milkconsisting of vitamin D concentrate uniformly dispersed in cream.

8. A sterile vitamin D concentrate adapted for addition to whole milkconsisting of a vitamin D concentrate uniformly dispersed in evaporatedmilk.

ANDRE. E. BRIOD. BION R. EAST.

